Process of recovering by-products from distillery-slop.



ALADAR VON LASZLOFFY, OF PEOIR-IA, ILLINOIS.

Specification of Letters Patent.

Patented July 2?, 1915.

No Drawing. Original application filed August 25, 1911, Serial No.645,912. Divided and this application filed October 20, 1913. Serial No.796,149.

To all whom it may concern:

Be it' known that I, ALADAR VON LAsz- LOFFY, citizen of the UnitedStates, residing at Peoria, in the county of Peoria and State ofIllinois, have invented certain new and useful Improvements in Processesof Recovering By-Products from Distillery-Slop; and I do hereby declarethat the following is a full, clear, and exact description of theinvention, which will enable others skilled in the art to which itappertains to make and use the same.

This invention relates to the recovery of by-products from'distillery-slop and particularly to a process by which groups of saidbyproducts are separated from the slop and from each other. Its objectis to recover from distillery-slop separate groups of Icy-products bytreating said slop or preparations derived from distillery-slop with aplurality of solvents in successlon.

It is known that distillery-slop or vinasses contain a number ofvaluable products among which are glycerin, organic acids and fats.

I have described in copending patent applications methods of treatingdistilleryslop or preparations of the same w1th a solvent, for instancealcohol, the aim of'which is to separate a mixture of the products fromthe slop, this mixture being afterward separated into groups ofproducts, individual products being finally separated from the groups.

In the present process the distlllery slop or preparations of the sameare treated first with a solvent that dissolves but a small number ofby-products following which a different solvent is used to extract otherproducts, the by-products being divided into groups from the verybegmning of the treatment. This method of extraction, which may becharacterized as fractional extraction, facilitates the recovery of theindividual by-products in a state of greaterpurity. I

In making use of the general principle of fractional extraction of theby-products from distillery-slop I have found It most practical to usefirst a solvent which has a high fat dissolving power, that is, onethat,

will dissolve the largest possible amount of said fat but which solventwill not mix with glycerin. The typical fat solvents answer therequirements of this process and I have found those to be mosteconomical which besides dlssolving the fat, also dissolve the lacticand the succinic acids, the separation of the fat from these organicacids being afterward very easily effected. Such solvents may be, forinstance, ether, chloroform, benzol, benzin, other hydrocarbons, thechlorderivates of hydrocarbons or mixtures of them having the describedproperty to some degree and it may be stated that the greater theaflinity of the solvent for water the more quickly it will extract theorganic acids, although the extracted products will be less pure. Theresidue resulting from the extraction through the use of the firstsolvent is treated with another solvent, as for instance with an alcoholor mixtures thereof with other solvents, but wherein the character ofthe alcohol predominates. By extracting said residue with this form ofsolvent a new solution is obtained containing principally glycerin,besides other substances. It is obvious that the fractional extractioncan be extended further by treating the residue of the second extractionwith still another solvent, for instance with an alcohol-water-mixture,or mixtures.

Either the whole slop or parts of the same may be treated in thedescribed manner, and the slop or its parts may be changed in form forthe extraction as by evaporating, drying, or mixing it with an absorbentmaterial, or other physical or chemical agents may be used. In referringto preparations of distillery-slop or mixtures of substances derivedfrom distillery slop I mean the various forms into which the slop orparts of the slop containing the by-products may be changed by physicalor chemical means.

While the whole slop may be treated with solvents by the process setforth, it is of course more practical to bring the by-products into amore concentrated form by eliminating water or other parts of the slopto reduce the volume to be treated.

The following will set forth the preferred manner of practising thepresent process and will also serve to better explain the generalprinciple of said process: 30,000 gallons of distillery-slop whichrepresent the residue of distillation of fermented distillerymashderived from 1,000 bushels of grain, are separated by any well known'means into a solid part and a liquid part. The liquid part isconcentrated in a vacuum-evaporator and the resulting syrupy-slop ismixed with the solid part of the slop after which the mixture is dried.This dried slop is now reduced to a granular form and placed in asuitable extraction apparatus. Such an apparatus may consist of apereolator in which the dried slop can be treated with the solvent, anda still in which the solution coming from the percolator is boiled,'anda reflex-cooler that condenses the vapors arising from the still; thecondensed solvent being returned to the percolator. Ethyl ether orsimilar solvent to the amount of substantially the volume of that of thedried slop is placed in the still and when caused to boil its vaporafter passing into the reflex-cooler percolates through the dried slopand returns to the still. This operation is made continuous or until theslop is practically exhausted of the organic acids. The solution inthestill is now Withdrawn and contains fat and lactic and succinic acids-ina state of high purity. The still is now filled with alcohol which isboiled and the resulting alcohol-vapor arises into the cooler where itis condensed and made to pass through the previously treated slop whichnow naturally contains a large quantity of ether. The mixture of alcoholand ether percolates through the material back into the still and againbeing sent to and through the material as before. The new solution inthe still is of a darker color than that obtained in the first treatmentwith tive amount of protein therein and it represents therefore avaluable concentrated cattle-feed.

. The treatment of the two solutions of byproducts obtained by theprocess shown in this example do not form a part of the presentapplication but are described and claimed in separate copendingapplications and the subject matter of this application is divided frommy former application for a process of recovering byproducts fromdistillery slop, Serial No. 645,912 filed in the U. S. Patent Office onthe 25th day of August 1911. a 7

By the use of the term distillery slop I means the residue ofdistillation obtained in the manufacture of alcohol from any rawmaterial used in the manufacture of alcohol.

Having described my invention I claim 1. The process of recovering aplurality of solutions of by-pr'oducts from a mixture of substancesderived from distillery slop consisting in treating said'mixture ofsubstances first with a fat-solvent capable of dissolving lactic acidand succinic acid and which has a tendency to repel glycerin, separatingthe solution resulting from this treatment from the residue, thentreating the residue with an alcoholic solvent, and again separating thesolution from the insoluble part.

2. The process of recovering a plurality of solutions of by-productsfrom a mixture of substances derived from distillery-slop consisting,first, in passing through a concentrated mixture of the same a solventcapable of dissolving fat and lactic and succinic acids and having atendency to repel glycerin, and, second, passing an alcoholic solventthrough the said concentrated mixture.

In testimony whereof I affix my signature, in presence of two Witnesses.

ALADAR VON LASZLOFFY.

Witnesses:

L. E. SUTHERLAND, L. M. THURLOW.

